QuEChERS-气相色谱-质谱联用法同时测定水产品中6种丁香酚类麻醉剂的残留量  

Determination of 6 kinds of eugenol derivatives residues in aquatic products by QuEChERS-gas chromatography-mass spectrometry

作　　者：黄武 李红权 刘建芳 高平 徐金龙 唐媛媛 李军 

机构地区：[1]湛江出入境检验检疫局检验检疫技术中心,湛江524001 [2]湛江市食品药品检验所,湛江524048

出　　处：《食品安全质量检测学报》2018年第2期422-428,共7页Journal of Food Safety and Quality

基　　金：广东检验检疫局科技项目(2016GDK30);国家质量监督检验检疫总局科技项目(2015IK058);湛江市财政资金科技专项(2012E0202)~~

摘　　要：目的建立Qu ECh ERS-气相色谱-质谱联用法同时测定水产品中6种丁香酚类麻醉剂残留量的分析方法。方法样品采用乙腈超声提取、基于Qu ECh ERS方法净化、RTX-5MS(25 m×0.25 mm,0.25μm)毛细管柱分离后,采用SIM模式检测,外标法定量。结果 6种丁香酚类麻醉剂在5.0~100μg/L范围内具有良好的线性关系,相关系数为0.9921~0.9995;对于5.00 g样品方法的检出限(limit of detection,LOD)为1.0~2.0μg/kg,定量限(limit of quantitation,LOQ)为2.5~5.0μg/kg;10、20、80μg/kg添加水平的加标实验中,平均回收率范围为73.2%~101.8%,相对标准偏差(relative standard deviation,RSD)为3.4%~13.6%。结论本方法具有操作简便、快速、灵敏度高、实用性强等特点,符合丁香酚类麻醉剂残留分析要求。Objective To establish a method for the simultaneous determination of 6 kinds of eugenol derivatives residues in aquatic products by QuEChERS-gas chromatography-mass spectrometry. Methods The samples were ultrasonic extracted by acetonitrile and purified by a modified Qu ECh ERS method. The target compounds were separated on RTX-5 MS column（25 m×0.25 mm, 0.25 μm） and detected by SIM mode. External standard method was applied for quantitative analysis. Results The linear range was from 5.0 to 100 μg/L with good correlation coefficients（r=0.9921~0.9995） for 6 kinds of eugenol derivatives. The limits of detection（LODs） and limits of quantitation（LOQs） were 1.0~2.0 μg/kg and 2.5~5.0 μg/kg for all compounds based on a 5.0 g sample. When the spiked concentrations were 10, 20 and 80 μg/kg, the average recoveries were in the range of 73.2%~101.8% with the relative standard deviations（RSDs） of 3.4%~13.6%. Conclusion This method is simple, quick, highly sensitive and practical and it can meet the requirements of residual analysis.

关 键 词：Qu ECh ERS 气相色谱-质谱法 丁香酚类化学物 水产品 渔用麻醉剂 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]